Dispersive liquid-liquid microextraction method of heavy metal ions by using alkyl carboxylic acid as extracting agent

A technology of heavy metal ions and alkyl carboxylic acids, applied in liquid solution solvent extraction, preparation of test samples, etc., can solve problems such as limited types of chelating agents and chelating efficiency, poor stability of chelating agents, and increased method complexity. Achieve the effect of low cost, less organic solvent and simple device

Inactive Publication Date: 2014-02-12
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
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AI Technical Summary

Problems solved by technology

Due to the introduction of the chelation reaction step before the extraction, the process takes a long time, the types of chelating agents and th

Method used

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  • Dispersive liquid-liquid microextraction method of heavy metal ions by using alkyl carboxylic acid as extracting agent
  • Dispersive liquid-liquid microextraction method of heavy metal ions by using alkyl carboxylic acid as extracting agent
  • Dispersive liquid-liquid microextraction method of heavy metal ions by using alkyl carboxylic acid as extracting agent

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Embodiment 1

[0036] Use mercuric chloride or mercuric nitrate crystals to configure Hg concentrations of 0, 1.0, 2.0, 4.0, 6.0, 8.0, 10.0ppb (micrograms per liter) respectively 2+ Aqueous solutions (respectively as standard samples) were enriched by using dispersion liquid-liquid microextraction method, the steps are as follows: first add 200mL Hg 2+ For the standard sample, heat the sample to 50°C and adjust the pH to 5; pre-mix 150 μL dodecanoic acid extractant and 3 mL methanol dispersant; quickly inject the mixed dodecanoic acid and methanol into the sample with a syringe to Stir rapidly at 1000r / min for 2min to form an emulsified system; place the sample in an ice bath for 10min; filter and separate the solidified dodecanoic acid; add 1mL of methanol to dissolve all the separated dodecanoic acid, and then add 2mL of 500μM rhodamine B Derivative rhodamine B thiospirolactone in acetonitrile solution, mixed well and then detected by fluorescence spectrometer.

[0037] Spectral condition...

Embodiment 2

[0039] Use nickel chloride crystals to configure Ni with concentrations of 50.0, 100.0, 150.0, 200.0, 250.0, 300.0, 350.0, 400.0ng / L 2+ Aqueous solutions (respectively used as water samples) were enriched by dispersion liquid-liquid microextraction method. The steps are as follows: first, add 100mL water sample to the extraction bottle, and place the extraction bottle in a water bath at 40°C; Mix with ethanol, quickly pour the mixture into the extraction bottle with a pipette, shake for 5 minutes, place the extraction bottle in an ice bath for 5 minutes, filter and separate n-decanoic acid; heat to 40°C, melt the extraction phase to obtain 150 μL n-decanoic acid, 20 μL was injected into electrothermal atomic absorption spectroscopy (ETAAS) for analysis. The initial concentration Caq of nickel ions in the aqueous phase sample was plotted against the concentration Cor of nickel ions in the 150 μL n-decanoic acid extraction phase separated by filtration. It was found that the lin...

Embodiment 3

[0041]Pb with concentration of 20.0, 60.0, 100.0, 140.0, 180.0, 220.0, 260.0ng / L is prepared with lead chloride crystal 2+ Aqueous solutions (respectively used as water samples) were enriched by using dispersion liquid-liquid microextraction method, the steps are as follows: first, add 100mL water sample to the extraction bottle, and place the extraction bottle in a water bath at 30°C; Mix with acetone, quickly inject the mixture into the extraction bottle with a syringe, and stir rapidly at 1000r / min for 2 minutes to form an emulsified system; place the extraction bottle in an ice bath for 5 minutes, filter and separate the extract phase and heat to 30°C to obtain 150 μL n-nonyl acid; 15 μL was injected into atomic fluorescence spectroscopy (AFS) for analysis. The method for Pb 2+ The enrichment factor is 350 times and the detection limit can reach 10ng / L. The peak height has a good linear relationship with the sample concentration in the concentration range of 20-260ng / L.

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Abstract

The invention provides a dispersive liquid-liquid microextraction method of heavy metal ions by using an alkyl carboxylic acid as an extracting agent. The method comprises steps of heating a sample making the temperature of the sample higher than the melt point of the alkyl carboxylic acid; mixing the alkyl carboxylic acid extracting agent and a dispersant; adding the mixture of the extracting agent and the dispersant into the sample to form an emulsion; cooling to solidify the extracting agent; and separating the solidified extracting agent for detection. The alkyl carboxylic acid in the method is used as a complexing agent and the extracting agent simultaneously. The method has less organic solvent types, small using amount of the organic solvents, short extraction time, high enrichment capability and simple operation. An elution step in solid-state microextraction, and a centrifugal separation step in traditional liquid-liquid microextraction are omitted. The method provided by the invention is a low-cost, simple and efficient sample pretreatment technology, and can extract the heavy metal ions in a water sample rapidly.

Description

technical field [0001] The invention relates to a dispersion liquid-liquid micro-extraction method, in particular to a heavy metal ion dispersion liquid-liquid micro-extraction method using an alkyl carboxylic acid as an extraction agent, and belongs to the technical field of material separation and analysis. Background technique [0002] Water is one of the important resources for human survival, but with the influence of human activities, more and more pollutants enter the water environment, among which heavy metal pollution is a very important category. Among them, the heavy metal elements entering the water body through various channels are difficult to degrade, easy to accumulate, irreversible, highly toxic, slow to metabolize and easy to be bio-accumulated in the environment, which has caused many problems for the environment and human health for many years. Therefore, heavy metal ion pollution in water has increasingly become the focus of attention. [0003] Due to t...

Claims

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Application Information

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IPC IPC(8): B01D11/04G01N1/34
Inventor 关亚风刘静吴大朋
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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